Hydrochloric Acid → HCID 22326703、化合物

HRID 896294ノート

反応式

HRID 896294 の反応式
C([N:4]1[C:12]2[C:7](=[C:8]([O:13][CH2:14][CH2:15][Cl:16])[CH:9]=[CH:10][CH:11]=2)[CH:6]=[N:5]1)(=O)C.Cl>CO>[Cl:16][CH2:15][CH2:14][O:13][C:8]1[CH:9]=[CH:10][CH:11]=[C:12]2[C:7]=1[CH:6]=[N:5][NH:4]2

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 22350151HCID 22350151、化合物

生成物 1

HCID 22326703HCID 22326703、化合物収率 96.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
65 °C

実験手順

A stirred solution of 1-acetyl-4-(2-chloroethoxy)-indazole (1.50 g, 6.3 mmol) in methanol is treated with hydrochloric acid (6.3 ml, 1.0 M HCl in Et2O, 6.3 mmol) at room temperature, heated at 65° C. under nitrogen for 18 hr, cooled to room temperature and concentrated in vacuo. The resultant residue is neutralized with 1N NaOH (6.0 ml) and diluted with H2O and ethyl acetate. The phases are separated and the aqueous phase is extracted with ethyl acetate. The combined organic phases are washed with water and saturated NaCl, dried over Na2SO4 and concentrated in vacuo to afford the title product (1.2 g) as a yellow solid, identified by NMR and mass spectral analyses.

後処理

  1. temperaturecooled to room temperature
  2. concentrationconcentrated in vacuo
  3. additiondiluted with H2O and ethyl acetate
  4. customThe phases are separated
  5. extractionthe aqueous phase is extracted with ethyl acetate
  6. washThe combined organic phases are washed with water and saturated NaCl
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-72459e4268e746c3bdd005b7f200ed50
出典データセット
uspto-grants-2005_07
特許番号
US06919354B2

反応ノート

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